CRITCL Mass Spec – Sample Submission

Training Requests

All training request must be submitted as a service request in our online billing system, iLab. For directions on how to establish an iLab account, please see below.

Sample Submission

Samples should be submitted directly to Dr. Ehrmann in Caudill 052. If she is not available during your desired drop-off time, please place the samples in the file holder located on her office door. All samples must be accompanied by a service request in our online billing system, iLab. For directions on how to establish an iLab account, please see below.

Fill out sample submission form under the service request tab completely. You need only to complete one service request per submission; however, you must disclose sample information about all submitted samples in a single service request.

The more information you provide about the sample pre-analysis, the higher quality your mass spectrometry results will be.

iLab Access

You can gain access to the Department of Chemistry Mass Spectrometry Core Laboratory by clicking here

If at any point you encounter issues with functionality of the iLab website feel free to reach out the Core Director or UNC’s on-campus iLab team at coresupport@med.unc.edu

UNC-CH/Internal Clients

The Mass Spectrometry Core Laboratory at UNC is excited to start using an online system to streamline the process of ordering and billing for core service requests. All Core Lab users are required to complete a one-time registration as discussed below. Once you are registered, the system will enable you to place service requests, provide required approvals, and monitor progress.

How to Register for an Account:
To get started, you must register for an account:

In the upper-right-hand corner of the screen where it says, ‘Welcome UNC user, please click here to login or register,’ select the ‘click here’ link

You will be directed to an authentication page where you will need to enter your UNC credentials

Once you have entered your credentials, click the ‘Login’ button

You will be directed to an iLab Registration page where you will need to select your PI/Lab, and verify your contact information

Once your registration has been submitted, your PI will receive a notification that you have requested membership to their lab in iLab. They will need to approve your membership and assign any Account Number for your use.

To Create an Equipment Reservation:
Once you have been accepted into your PI’s lab and assigned Account Number, you can schedule equipment time.

At the upper right hand of the page where it says, ‘Welcome UNC user, click here to log in or register,’ select click here.

Enter your UNC Credential and password, and sign in.

Select the Request Services tab and click on the ‘Request Service’ button next to the service of interest.

You will be asked to complete a form before submitting the request to the core.

Your request will be pending review by the core. The core will review your request and either Agree to the work or they will ask for more information if needed.

External Clients

The UNC Department of Chemistry Mass Spectrometry Core Lab requires a one-time registration as discussed below. Once you are registered, the system will enable you to place service requests, provide required approvals, and monitor progress.

How to Register for an Account:

Complete the registration form on the sign-up page.

Receive a Welcome Email from iLab ,typically within one business day, with login credentials.

To Create a Service Request:
Using your iLab login credentials, you can place a service request.

Login Here using the ‘External UNC user?’ option.

Enter the credentials received in your welcome email from iLab.

Select the Request Services tab and click on the Request Service button next to the service of interest.

You will be asked to complete a form before submitting the request to the core.

Your request will be pending review by the core. The core will review your request and either Agree to the work or they will ask for more information if needed.

To Create an Equipment Reservation:
Using your iLab login credentials, you can place orders and schedule equipment time.

Login Here using the ‘External UNC user?’ option.

Enter the credentials received in your welcome email from iLab.

Select the Schedule Equipment tab and click on the View Schedule button next to the instrument of interest. Click and drag on the time frame you would like to schedule your reservation for.

A window will pop up that will allow you to verify your reservations details and provide payment information before saving the reservation.

For UNC PIs:

If you have researchers who use the core’s services, you may receive email requests from researchers wishing to join your group. The request email will have specific instructions on how to approve the request. In case you are interested in the process, we have pasted instructions below. If you would prefer to delegate these notifications/approvals to a financial manager, please email coresupport@med.unc.edu with your financial manager’s name & email.

Instructions:

Click here to log-in: Core External URL

You will use your UNC credentials to log into iLab

Once logged in, look for the link in the left hand menu that says ‘my labs’. Hover-over and select your lab.

Set the auto-approval amount if you do not wish to approve service requests below a certain dollar amount. To do this, select the ‘Members’ panel and enter a dollar amount in the ‘Auto Pre-Approval’ amount and click ‘save settings.’

To approve lab membership requests, select the ‘Membership Requests & Account Numbers’ tab. New membership requests will show at the top of this page. Click “Approve” to accept a member into your lab. Click “Reject” if they are not a member of your lab.

To assign an Account Number to a member of your lab, find the member in the above list where it says, ‘Manage Account Numbers.’ Select the checkbox/es to the right of their name for the Account Number/s you wish to assign them.

When submitting samples, please follow these guidelines for each type of sample that you would like us to analyze.

Electrospray Ionization – ESI
Samples can be either liquid or solid. Samples submitted in solution should be dissolved in suitable solvent at a concentration of 100 µM. Solvents must be specified, or solubility information should be provided. Solvents recommended are methanol and acetonitrile. Solvents that should be avoided are DMSO, THF, and DMF. All buffers and salts should be avoided.

ICP-MS Liquid Analysis
It is ideal that you utilize metal free tubes, tips, bottles, and other materials for ICP-MS analysis.
All samples will be completely digested in acid and diluted in 18.2 MΩ water prior to running on the ICP. Refer to the Inorganic Ventures Sample Preparation site for specifics on dissolving your element of interest. You will need trace metal grade nitric acid, HNO3, and in some cases a 1:1 mixture of nitric acid, HNO3, and hydrochloric acid, HCl. Some metals require hydrofluoric acid, HF, to dissolve, but please use caution when working with HF.

Microwave Digestion
It is ideal that you utilize metal free tubes, tips, bottles, and other materials for ICP-MS analysis.
If you are having trouble digesting your samples using a conventional hot plate, we can utilize our MARS microwave digestion system to aid in this process. Please consult our staff for assistance in how to program the microwave system to effectively conduct your digestion.

Laser Ablation
Samples do not need surface preparation, but data quality is improved considerably if the samples are polished. Samples should be clean, dry and where possible any carbon coating from previous electron probe microanalysis should be removed. Any gold coating on samples previously imaged by scanning electron microscopy or ion probe analysis must be removed thoroughly. Residues of gold coating can severely affect LA-ICP-MS data quality.

Sample preparation
Different types/size geological sample can be accommodated in our Laser Ablation system because of its in-house designed sample holder. There are several requirements for the samples:
– Polished 1 or ½ inch epoxy disc
– Standard, 7.3 x 2.5 cm, sample thin-section / or grains of sample,oraminifera shells, attached to the glass slide using carbon tape
– Semi-flat/polished slab of rocks/coral speleothems which dimensions no large than 13.8 cm by 8 cm or combination of smaller blocks with same total area. (13.5x3cm –preferable)

Standards
We have a set of NIST glass, 610-614, for trace metal analyses of no ‘matrix’ challenging samples. We also have a large collection of well-characterised carbonate standards, trace metals, Mg isotopes, U/Th, B isotopes.

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Safety

The Department of Chemistry is committed to providing a safe and productive environment for both students and staff. The highest standards of scholarship can only be attained in an environment that emphasizes a culture of safety. All laboratories are required to adhere to safety rules and regulations.

Diversity

At the Department of Chemistry, we feel strongly that diversity is crucial to our pursuit of academic excellence, and we are deeply committed to creating a diverse and inclusive community. We support UNC's policy, which "affirms the University's commitment to providing an inclusive and welcoming environment that is free from discrimination on the basis of age, color, creed, disability, gender, gender expression, gender identity, genetic information, national origin, race, religion, sex, sexual orientation or veteran status."